Derivatives of celeboxib, use thereof and preparation thereof
a celeboxib and derivative technology, applied in the field of celeboxib derivatives, can solve the problems of limited clinical use, many chemotherapeutic drugs also produce undesirable side effects in patients, etc., and achieve the effect of reducing adverse side effects
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example 1
4-(3-tert-Butyl-5-(4-methoxyphenyl)-4,5-dihydro-1H-pyrazol-1-yl)benzoic acid (1)
[0052]Yield: 30% white powder; m.p.: 208.9° C.; TLC: Rf=0.78 (CH2Cl2:CH3OH, 5:1); 1H-NMR: δ 7.67 (d, J=9.01, Hz, 2H, ArH), 7.12 (d, J=8.73 Hz, 2H, ArH), 6.84-6.89 (m, 4H, ArH), 5.30 (dd, J=11.66, 5.00 Hz, 1H, H5), 3.70 (s, 3H, OCH3), 3.55 (dd, J=17.70, 11.70 Hz, 1H, H4b), 2.72 (dd, J=17.70, 5.04 Hz, 1H, H4a), 1.18 (s, 9H, tBu); 13C-NMR: δ 27.86, 33.55, 42.56, 55.00, 61.66, 111.34, 114.33, 118.87, 126.78, 130.70, 134.11, 147.83, 158.45, 161.46, 167.26; IR (cm−1): 2600-3200 (—OH), 1660 (—CO—); MS (ESI): 353.22 (M++1), 351.19 (M+−1) C21H24N2O3; Purity (HPLC): 96.2%
example 2
4-(3-tert-Butyl-5-(4-nitrophenyl)-4,5-dihydro-1H-pyrazol-1-yl)benzoic acid (2)
[0053]Yield: 35% yellow powder; m.p.: 245.2° C.; TLC: Rf=0.81 (CH2Cl2:CH3OH, 5:1); 1H-NMR: δ 12.06 (brs, 1H, COOH), 8.06 (d, J=8.78, Hz, 2H, ArH), 7.54 (d, J=8.94 Hz, 2H, ArH), 7.32 (d, J=8.78 Hz, 2H, ArH), 6.70 (d, J=8.89 Hz, 2H, ArH), 5.42 (dd, J=11.88, 5.14 Hz, 1H, H5), 3.50 (dd, J=17.81, 11.93 Hz, 1H, H4b), 2.64 (dd, J=17.82, 5.15 Hz, 1H, H4a), 1.03 (s, 9H, tBu); 13C-NMR: δ 27.81, 33.58, 42.21, 61.56, 111.42, 119.51, 124.28, 127.06, 130.86, 146.85, 147.52, 149.64, 161.60, 167.16; IR (cm−1): 2600-3200 (—OH), 1678 (—CO—), 2966 (C—H); MS (ESI): 366.22 (M+−1) C20H21N3O4; Purity (HPLC): 99.81%
example 3
4-(3-tert-Butyl-5-(3-nitrophenyl)-4,5-dihydro-1H-pyrazol-1-yl)benzoic acid (3)
[0054]Yield: 50%; Yellow powder; m.p.: 235.4° C.; TLC: Rf=0.36 (CH2Cl2:CH3OH, 100:2); 1H-NMR: δ 8.11 (d, J=9.5 Hz, 2H), 7.67 (dd, J=16.8, 7.5 Hz, 4H), 6.89 (d, J=7.9 Hz, 2H), 5.60 (dd, J=11.52, 4.69 Hz, 1H), 3.65 (dd, J=17.9, 11.7 Hz, 1H), 2.84 (dd, J=17.99, 4.40 Hz, 1H), 1.19 (s, 9H); IR (cm−1): 2800-3200 (—OH), 1660 (—CO—); MS (ESI): 367.65 (M+) C20H21N3O4; Purity (HPLC): 97.6%.
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